CN110183555B - Preparation method of mulberry-shaped europium-doped barium polyacrylate powder - Google Patents
Preparation method of mulberry-shaped europium-doped barium polyacrylate powder Download PDFInfo
- Publication number
- CN110183555B CN110183555B CN201910454637.0A CN201910454637A CN110183555B CN 110183555 B CN110183555 B CN 110183555B CN 201910454637 A CN201910454637 A CN 201910454637A CN 110183555 B CN110183555 B CN 110183555B
- Authority
- CN
- China
- Prior art keywords
- solution
- mulberry
- hydrothermal reaction
- preparation
- polyacrylate powder
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- 229910052788 barium Inorganic materials 0.000 title claims abstract description 19
- 229920000058 polyacrylate Polymers 0.000 title claims abstract description 19
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 239000000843 powder Substances 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 17
- 239000000243 solution Substances 0.000 claims abstract description 16
- 229920002125 Sokalan® Polymers 0.000 claims abstract description 15
- 239000004584 polyacrylic acid Substances 0.000 claims abstract description 15
- 239000007864 aqueous solution Substances 0.000 claims abstract description 13
- 239000011259 mixed solution Substances 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 5
- 238000001914 filtration Methods 0.000 claims abstract description 5
- 239000002244 precipitate Substances 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims abstract description 3
- 238000005303 weighing Methods 0.000 claims abstract description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 238000000034 method Methods 0.000 claims 2
- 239000000047 product Substances 0.000 abstract description 6
- 238000009776 industrial production Methods 0.000 abstract description 2
- 238000005424 photoluminescence Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 6
- 229910052761 rare earth metal Inorganic materials 0.000 description 4
- 150000002910 rare earth metals Chemical class 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 2
- 239000008204 material by function Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 235000008708 Morus alba Nutrition 0.000 description 1
- 240000000249 Morus alba Species 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000000295 emission spectrum Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000000695 excitation spectrum Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 description 1
- 239000002455 scale inhibitor Substances 0.000 description 1
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F8/00—Chemical modification by after-treatment
- C08F8/44—Preparation of metal salts or ammonium salts
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/06—Luminescent, e.g. electroluminescent, chemiluminescent materials containing organic luminescent materials
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K2211/00—Chemical nature of organic luminescent or tenebrescent compounds
- C09K2211/14—Macromolecular compounds
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Luminescent Compositions (AREA)
Abstract
The invention provides a preparation method of mulberry-shaped europium-doped barium polyacrylate powder, which comprises the following steps: a. weighing Ba (NO)3)2Dissolving in water to obtain Ba (NO)3)2A solution; b. in Ba (NO)3)2Adding Eu (NO) into the solution3)3Uniformly stirring the solution and 50wt% of polyacrylic acid aqueous solution to obtain a mixed solution; c. placing the mixed solution in a reaction kettle, and carrying out hydrothermal reaction for 4-16 h at the temperature of 120-140 ℃; d. and filtering after the hydrothermal reaction is finished, and washing and drying the obtained precipitate to obtain mulberry-shaped europium-doped barium polyacrylate powder. The preparation method uses hydrothermal reaction, is simple, does not need high-temperature roasting, and is suitable for large-scale industrial production. The mulberry-shaped barium polyacrylate powder is obtained by controlling conditions such as hydrothermal reaction temperature, and the product has uniform and stable size, controllable appearance, larger specific surface area and good photoluminescence performance.
Description
Technical Field
The invention relates to the technical field of luminescent material preparation, in particular to a preparation method of mulberry-shaped europium-doped barium polyacrylate powder.
Background
Since the new century, people pay more attention and attention to functional materials, and the preparation of new materials becomes one of the key points of research. In the development of rare earth functional materials, rare earth luminescent materials are particularly attractive. Rare earth metals have spectral properties incomparable with common elements due to their special electron shell structures.
Polyacrylic acid is a colorless or yellowish liquid, can form a stable compound with metal ions, and is commonly used as a scale inhibitor and a water absorbent. At present, the preparation method of low molecular weight sodium polyacrylate is reported in the published domestic patent documents (such as the document numbers CN1106355C, CN1141262C, CN101172718A and the like), the preparation method of the barium polyacrylate is not reported at present, the rare earth luminescent polyacrylate luminescent material has good application prospect in the luminescent field, and the research of a novel barium polyacrylate luminescent material and the preparation method thereof have important significance.
Disclosure of Invention
The invention aims to provide a preparation method of mulberry-shaped europium-doped barium polyacrylate powder, which aims to solve the problems of few varieties and unsatisfactory comprehensive performance of the existing polyacrylate luminescent materials.
The purpose of the invention is realized by the following technical scheme: a preparation method of mulberry-shaped europium-doped barium polyacrylate powder comprises the following steps:
a. weighing Ba (NO)3)2Dissolving in water to obtain Ba (NO)3)2A solution;
b. in Ba (NO)3)2Adding Eu (NO) into the solution3)3Uniformly stirring the solution and 50wt% polyacrylic acid aqueous solution to obtain a mixed solution, wherein Ba (NO) is contained in the mixed solution3)2Eu (NO) dosage3)3The dosage of the polyacrylic acid aqueous solution is 50wt%, and the dosage of the polyacrylic acid aqueous solution is =1 mol: 0.0067-0.066 mol: 1-5 g;
c. placing the mixed solution in a reaction kettle, and carrying out hydrothermal reaction for 4-16 h at the temperature of 120-140 ℃;
d. and filtering after the hydrothermal reaction is finished, and washing and drying the obtained precipitate to obtain mulberry-shaped europium-doped barium polyacrylate powder.
Further, in step b, Ba (NO)3)2Eu (NO) dosage3)3The dosage of the polyacrylic acid aqueous solution is 50wt%, and the dosage of the polyacrylic acid aqueous solution is =1 mol: 0.0067-0.066 mol: 2 g.
Further, in the step c, the hydrothermal reaction temperature is 140 ℃ and the reaction time is 12 h.
The preparation method uses hydrothermal reaction, is simple, does not need high-temperature roasting, has low energy consumption and no pollution to the environment, and is suitable for large-scale industrial production. The mulberry-shaped barium polyacrylate powder is obtained by controlling the hydrothermal reaction temperature, has uniform and stable size, controllable appearance, larger specific surface area and good photoluminescence performance.
Drawings
FIG. 1 is a scanning electron micrograph of a product obtained in example 1 of the present invention.
FIG. 2 shows the excitation spectrum and the emission spectrum of the product obtained in example 1 of the present invention.
FIG. 3 is a scanning electron micrograph of a product obtained in comparative example 1 of the present invention.
Detailed Description
The present invention will be described in detail with reference to specific examples.
Example 1
a. 1.241g of Ba (NO)3)2Dissolving in 20mL water to obtain Ba (NO)3)2A solution;
b. to the above solution was added 833. mu.L of 0.2mol/L Eu (NO)3)3The solution and 2g of 50wt% polyacrylic acid aqueous solution are uniformly stirred to obtain a mixed solution;
c. placing the mixed solution in a reaction kettle, and carrying out hydrothermal reaction for 12 hours at the temperature of 140 ℃;
d. and after the hydrothermal reaction is finished, filtering, washing and drying the precipitate to obtain the barium polyacrylate powder. The obtained product was characterized and the results are shown in fig. 1 and 2. As can be seen from figure 1, the sample has uniform and stable size, good dispersibility, mulberry-shaped appearance and diameter of about 5 μm.
Comparative example 1
a. 1.241g of Ba (NO)3)2Dissolving in 20mL water to obtain Ba (NO)3)2A solution;
b. to the above solution was added 833. mu.L of 0.2mol/L Eu (NO)3)3The solution and 2g of 50wt% polyacrylic acid aqueous solution are uniformly stirred to obtain a mixed solution;
c. placing the mixed solution in a reaction kettle, and carrying out hydrothermal reaction for 12 hours at the temperature of 160 ℃;
d. and after the hydrothermal reaction is finished, filtering, washing and drying the precipitate to obtain the barium polyacrylate powder. The scanning electron microscope image of the obtained powder is shown in fig. 3, and as can be seen from fig. 3, the appearance of the sample in this example is two-phase rather than mulberry, which indicates that the reaction conditions have a great influence on the appearance of the product.
Examples 2 to 4
The hydrothermal reaction time was varied (see Table 1, for details), other raw materials and conditions were the same as in example 1, and the test results are shown in Table 1.
Table 1:
examples 5 to 8
The amount of 50wt% aqueous polyacrylic acid solution (see Table 2) was changed, and other raw materials and conditions were the same as in example 1, and the test results are shown in Table 2.
Table 2:
Claims (3)
1. a preparation method of mulberry-shaped europium-doped barium polyacrylate powder is characterized by comprising the following steps:
a. weighing Ba (NO)3)2Dissolving in water to obtain Ba (NO)3)2A solution;
b、in Ba (NO)3)2Adding Eu (NO) into the solution3)3Uniformly stirring the solution and 50wt% polyacrylic acid aqueous solution to obtain a mixed solution, wherein Ba (NO) is contained in the mixed solution3)2Eu (NO) dosage3)3The dosage of the polyacrylic acid aqueous solution is 50wt%, and the dosage of the polyacrylic acid aqueous solution is =1 mol: 0.0067-0.066 mol: 1-5 g;
c. placing the mixed solution in a reaction kettle, and carrying out hydrothermal reaction for 4-16 h at the temperature of 140 ℃;
d. and filtering after the hydrothermal reaction is finished, and washing and drying the obtained precipitate to obtain mulberry-shaped europium-doped barium polyacrylate powder.
2. The method of claim 1, wherein in step b, Ba (NO) is added to the powder3)2Eu (NO) dosage3)3The dosage of the polyacrylic acid aqueous solution is 50wt%, and the dosage of the polyacrylic acid aqueous solution is =1 mol: 0.0067-0.066 mol: 2 g.
3. The method for preparing the mulberry-like europium-doped barium polyacrylate powder as claimed in claim 1, wherein in the step c, the hydrothermal reaction temperature is 140 ℃ and the reaction time is 12 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910454637.0A CN110183555B (en) | 2019-05-29 | 2019-05-29 | Preparation method of mulberry-shaped europium-doped barium polyacrylate powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910454637.0A CN110183555B (en) | 2019-05-29 | 2019-05-29 | Preparation method of mulberry-shaped europium-doped barium polyacrylate powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110183555A CN110183555A (en) | 2019-08-30 |
| CN110183555B true CN110183555B (en) | 2021-06-29 |
Family
ID=67718563
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910454637.0A Expired - Fee Related CN110183555B (en) | 2019-05-29 | 2019-05-29 | Preparation method of mulberry-shaped europium-doped barium polyacrylate powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110183555B (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03115435A (en) * | 1989-09-29 | 1991-05-16 | Nippon Valqua Ind Ltd | Production of molded article of nitrile rubber |
| US6689823B1 (en) * | 1999-03-31 | 2004-02-10 | The Brigham And Women's Hospital, Inc. | Nanocomposite surgical materials and method of producing them |
| CN101096309A (en) * | 2006-06-30 | 2008-01-02 | 中国科学院合肥物质科学研究院 | Zinc oxide pressure-sensitive ceramic and preparation method thereof |
| CN104741135A (en) * | 2013-12-31 | 2015-07-01 | 西北大学 | Preparation method of barium sulfate-carbon aerogel composite support supported palladium catalyst |
| CN105237911A (en) * | 2015-11-01 | 2016-01-13 | 吕小方 | Heat stabilizer |
| CN109735333A (en) * | 2019-01-15 | 2019-05-10 | 河北大学 | One kind mixing europium calcium molybdate raw powder's production technology and application |
-
2019
- 2019-05-29 CN CN201910454637.0A patent/CN110183555B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03115435A (en) * | 1989-09-29 | 1991-05-16 | Nippon Valqua Ind Ltd | Production of molded article of nitrile rubber |
| US6689823B1 (en) * | 1999-03-31 | 2004-02-10 | The Brigham And Women's Hospital, Inc. | Nanocomposite surgical materials and method of producing them |
| CN101096309A (en) * | 2006-06-30 | 2008-01-02 | 中国科学院合肥物质科学研究院 | Zinc oxide pressure-sensitive ceramic and preparation method thereof |
| CN104741135A (en) * | 2013-12-31 | 2015-07-01 | 西北大学 | Preparation method of barium sulfate-carbon aerogel composite support supported palladium catalyst |
| CN105237911A (en) * | 2015-11-01 | 2016-01-13 | 吕小方 | Heat stabilizer |
| CN109735333A (en) * | 2019-01-15 | 2019-05-10 | 河北大学 | One kind mixing europium calcium molybdate raw powder's production technology and application |
Non-Patent Citations (3)
| Title |
|---|
| Fourier-Transfrom Infrared Studies of Ionomeric Blend and Ionic Aggregation;Sang Kong Lee，等;《Bull Korean Chem Soc》;19861231;第7卷(第4期);第267-271页 * |
| Strategy to enhance the red-emission of CaWO4:Eu3+ phosphors assisted by poly acrylic acid;Xiaoqing Guo，等;《Solid State Science》;20191130;第97卷;第105979号 * |
| 掺钡纳米氧化镁及其负载钌基氨合成催化剂的改性研究;夏庆华，等;《中国优秀硕士学位论文全文数据库工程科技I辑》;20150815(第8期);B015-49 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN110183555A (en) | 2019-08-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Qiu et al. | Effectively enhancing blue excitation of red phosphor Mg2TiO4: Mn4+ by Bi3+ sensitization | |
| Paulraj et al. | Photoluminescence efficiencies of nanocrystalline versus bulk Y2O3: Eu phosphor—revisited | |
| CN109678506A (en) | A kind of preparation method of erbium oxide crystalline ceramics | |
| CN105018087B (en) | Eu3+Adulterate laminated perovskite structure La2CuO4The preparation method of fluorescent powder | |
| Han et al. | Photoluminescence properties of Y3Al5O12: Eu nanocrystallites prepared by co-precipitation method using a mixed precipitator of NH4HCO3 and NH3· H2O | |
| CN108728078B (en) | Preparation method and application of NaYF4 Gd/Tm/Er @ CdTe | |
| CN110183555B (en) | Preparation method of mulberry-shaped europium-doped barium polyacrylate powder | |
| CN101831292A (en) | Strontium aluminate luminous material and controllable synthesis method thereof | |
| CN103627391B (en) | Preparation method of LaB3O6: Eu3<+> luminescent material | |
| CN100529012C (en) | Red solid solution Sr-In-Ti phosphor and its preparing method | |
| CN109666482A (en) | A kind of preparation method of rare-earth-doped fluoride up-conversion luminescence nano-powder | |
| CN109810706B (en) | Preparation method of hydrangea-like europium-doped calcium molybdate powder | |
| CN104845615A (en) | Rare-earth doped beta-phase Sr2SiO4 nano-powder and preparation method therefor | |
| CN104073252A (en) | Preparation method of ZnB2O4:Eu<3+> luminescent material | |
| Du et al. | Facile combustion synthesis of novel CaZrO 3: Eu 3+, Gd 3+ red phosphor and remarkably enhanced photoluminescence by Gd 3+ doping | |
| CN103950913A (en) | Preparation method of water-soluble fluorescent carbon nanopowder | |
| CN109233829B (en) | Magnesium erbium ytterbium three-doped sodium niobate and preparation method and application thereof | |
| CN102061168A (en) | Method for improving luminosity of europium-doped yttrium oxide red fluorescent powder | |
| CN101333441A (en) | Method for preparing Ce<3+> doped lutetium aluminium garnet nanometer ceramic luminescent powder | |
| CN105481000A (en) | SrY2O4 nanoneedle and preparation method thereof | |
| CN111018517A (en) | Multifunctional ferroelectric ceramic material and preparation method thereof | |
| CN1861737A (en) | Preparation process of long afterglow luminescent powder superfine powder of alkaline earth aluminate by codeposition/microwave method | |
| CN115181568B (en) | Synthesis of multi-layer core-shell structure composite nano dual-mode luminescent material | |
| CN116239381B (en) | Laser ceramic material capable of enhancing ion transformation inhibition capability and preparation method thereof | |
| CN102358836A (en) | High efficiency red phosphor powder and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20210629 |